Gaston guignard and andrfi h



(No Model.)

G. GUIGNARD 8; A. HEDOUIN. PROCESS OF AND APPARATUS FOR MANUFACTURINGALCOHOL.

No. 436,735. Patented Sept. 16,1890Q EJI MIL A @515 (ll/01 140 [UNITEDSTATES, PATENT OFFICE;

GASTON GU-IGNARD AND Anyone nnnoun'v, or'rnnrs, FRANCE.

PRocEsso'F AND APPARATUS FOR MnNuFAcruRme. ALCQHbLL:

srncmicn'rron forming part of Letters Patent No. 436,735,

' Application filed January 28,1890- Serial No. 338,435. (No model.)

.1'0 all whom, it may concern:

Be it known that we, GASTON GUIGNARD and ANDRE Hnnourmcitizens of theRepuh lie of France, and residents of Paris, in said Republic, haveinvented certain new and useful Improvements in Processesot andApparatus for the Manufacture of Alcohols, of

which the following specilication is a full,

clear, and exact description. 7

This invention rel tes to the manufacture of alcohols by. fermentationand distillation,

and has for its object particularly the manufracture of the same in apure state by avoiding the production with the alcohol of nudesir-ableforeign bodies.

The divers processes heretofore employed have involved the fermenting ofthe juices in presence of the air, and consequently also in the presenceof all-the germs contained therein. If, now, the impurities in alcoholsthus made (which impurities it is the object of variousold and modernprocesses to remove in order toproduce pure alcohol) be ex'amine'd froma chemical point of view, it will be found that they are largely, if notwholly, produced by either the germs existing in the airor germscontained in the impure yeast employed, or

' germs contained in the juices or liquors to be fermented themselves.These impurities here spoken of, whose destruction or transformation issought when the purification of alco- 1101 is, desired, are, first,aldehydes; second,

homologous alcohols higher than ethylicalcohol'; third, ethers; fourth,bases. It is known that the aldehydes are produced by the oxidation ofthe alcohols during the fermentation by the acetic ferment found in the[alcohols-are produced, first, bythe'action' juices orliquors to befermented. The higher of the butyric ferment, which decomposes" orconverts the suganthe glycerine, '&c., into butyric acid, .bntylicalcohol, carbonic acid,

hydrogen; second, by the purely chemical action of the nascent hydrogen,which gives by acting on the glucose, first, mannite, and, second, theseries of monatomic alcohols after 5 been ,hexylic alcoholf The organicacids contained in the juices or liquors to be fore mented give rise toodorous ethers, particularly when wines or vinous'liquids acidified witha mineral acid are distilled. Finally the albuminoid, matters, of theliquors, and even tact with u out of contact with ties indicated. Thisbeing so, it will be understood that such process gives a larger yieldand eifects an important economy,si noe pure alcohols are directlymanufactured. To pre-.

vent the production of the specified impuridated September 16, 1890'. IZ

already dead yeaste are therefore unavoidably 7 ties proceeding from thepresence of ferments in the air, in the juices or liquors, or in theimpure yeast, asalready stated, the opera tions are so carried on as toprevent from the commencement to the end of themanufacture theintroduction of any of these hurtful I ferments.

The new or improved process of,

manufacture rests, then, on the following principles: first,sterilization of the musts; second, aeration of the mustswithsterilized' air;

third, fermentation of the musts out of connsterilized-air by means of apure yeast-from the preparation of afldetermined and selected cell;fourth, maintenance of the temperature nearly constant during the fer--mentation; fifth, filtration of the wines after fermentation in filtersvso constructed that the and the yeast which they. hold remain I liquidsthe air and all germs-for eign to the yeast, and also for reasons to beexplained hereinafter; sixth, neutralization or slight uors; seventh,neutral or slightly alkaline liquors; *eilghth, a second distillationover an acid or equivalent alkalization of the fermented liqi a primarydistillationof; the

salt. By fermenting the sterilized musts out of contactwith the air bymeans of apure yeast the oxidizing action of the acetic fer-f ment andconsequently the destructionofa hols produced either bythe butyricferment n35 part of the alcohol formed is avoided. The formation also isavoided of the higher alco-;

r or by the action on the glucose of the nascent" sugar into butyricacid by the former and of a part of the alcohol into aldehyde and aceticI acid by the latter ferment. The two causes of the .production of acidarefthus avoided, and consequently the formation of ethers is avoidedalso. single matter of expense resulting from the bio of the yeast. Thealbuminoid matters of the liquors, or even, as has been said, thosecontained in the already dead cells of yeast, give on hydration .acids,ammonias, and amldo acids. The acids once produced, whatever theirsource, give rise to ethers, particularly when wines or vinous liquidsacidified with a'mineral acid are distilled.

According to the present invention the wines orvinous liquids aredistilled in a neu- 'tral or slightly alkaline condition in order toprevent this etherification and to destroy the ethersalready formed; butas the products of an ammoniacalnature arising from the decomposition ofthe albuminoid matter of the yeast or offthat contained in the liquorscan pass over in distillation a second distillation is or may benia'deover an. acid-salt or salt 1 .ca'pableof'forming adouble salt' withthese bodies.

duc'tionofethers{(acetates,

, Forthis purpose an acid-salt or salt K such as sulphate of alu ininamay be employed. To resume by the present invention the formationduringfermentation is avoided of, first, aldehydes; second, amylic,butyric, &c., alcohol; third,-a part of the acids. The pro- I abutyratesof ethyl, dqcmduring jthe disi illation of the wines orvl1i011siiquidsf ,avoided by making them "alkaline'duringjthatioperation. Finally to keep backthe ammon iacal products a seconddistillation of the alcohol from the former The followingis'adescription of the mode distillationis, if need be, made over anacidsalt, such as the ta'rt'rate of potash, or of soda, xor'oversnlphateof alumina.

or carrying the invention into efiect, refer- "[ence-beinghadt-o theaccompanying drawings, which form and in whichpart of thisspecification,

Figure I represents in sectional elevation a I general scheme ofapparatus for that purpose.

' Fig.1I is a sectional elevation, on a larger a similar detail ofthe'filter.

-scale, of the sterilizer for must; and Fig. III,

This apparatus also forms a part of theinv'ention.

Sterflizatiom-Sterilization of the juices or liquors to be fermented canbe obtained by one of the several known means. 'By preferencesterilization by superheating is em,-' ployed as simpleandconvenient.Filtration by porous walls may also be employed. The sterilization I bysuperheating' is effected by ,heating the liquors for twenty minutes to1 25- centigradefi For this purpose the liquors.

areplaced in a closed tank B and heated by.

There remains, however, a

direction to the movement of the juices. They are thus cooled to about20 centigrade. The coil 0 is itself previously sterilmay be connected.In a general way the apdivided by horizontal partitions which extendalternately from opposite sides nearly across the tank, and the coil 0is developed flatwise formed,- suitable connection being made with theportion of the-coil in the next compartment above and below. Thus a verylarge cooling surface is obtained.

Filtration-From the coil 0 the liquors pass, always out of contact withthe air, into a closed filter composed of the tank E, divided in two bythe filtering-cloth or filtering-diaphragm F. Prior to admitting thejuices or themain A*, the blow-off B being open, and when the air hasbeen expelled the said blowofi is closed and steam is retained in thetank under a pressure of about two kilogramsfor some time. Then thesteam-pipe R is closed and the pipe R for the admission of the liquor isopened. The condensation of the steam induces the filtration of theliquor through the filtering material F.

the aerating-vat G, filled with sterilized air, wherein they becomecharged with oxygen. The aerating apparatus is vco'mposed of a vat,

troduced through the pipe 3, terminating at the lower end in arose orsprinkler. They" fall on aseries of'diaphragms H of perforated fromcenter to circumference, the inclinationin adjacent diaphragms being inopposite directions. The aerating apparatus communicates by the pipe Iwith the steam-main A? aiid by the pipe K with the apparatus for sup.-plying sterilized air, (to be hereinafter described.) Fermentation.Fromthe aerator the liquors run into the fermenting-vat L, which to preventthe entrance of, the outside air. The vat is provided with a coil M,(movable like the coil A and similarly provided with and bottom of thevat,) through which cold Water may be circulated. On the bottom ofparatus preferred is composed of a tank D,

liquors the air is. expelled from the tank E by steam admit-ted throughthe pipe R from Aeration.-From the filter the liquors enter D, whereincold water circulates in inverse 'ized by steam. Two refrigeratingapparatus in each of the horizontal compartments thus at the upper partof which the liquors are insheet metal, which present a slightinclination has been previously sterilized, and which is I providedwithan hydraulic jointat the top stoning-boxes where it passes through thetop j communicating at one end with the steammain A*- through the pipe0, and at the other end through the pipe P with the apparatus forsupplying sterilized air. The cover of the vat is provided with a seriesof copper tubes Q, of small diameter, coiled into spiralform and closedeach-by a plug of asbestos, covered with oneof cotton. There are alsotwo pipes S and T terminating in roses or sprinklers within the vat, theformer S serving for the introduction of thesmusts and the latter 'I'for the pure yeast prepared outside in the small vat U of analogousconstruction. This yeast-vat is wholly of metal. It is first sterilized,and then a portion of the liquors from the aerator G is admittedthereiut-o through the pipe 8,. This portion of the liquors isfertilized with yeast cultivated outside with all the necessaryprecautions and tested before it is used for fertilization in order tobe certain of its purity. The yeast-vat is provided with an outlet Tsome distance from the bottom, in order that the yeast may bedrawn offwithout disturbing the leaven in the vat, so that the preparation of theyeast may be continuous. It is p or may be also provided with a pipedirectly at the bottom for drawing oif the whole contents. Lastly thevat U, like the fermentingvat L, is provided witha cooling-coil, (letterin this instance) inorder to maintain the temperature constant at thedesired degree.

d The pure yeast producedin the vat'U is filter is constituted byacylinder with conitransferred with the liquid which .has produceditthrough the. pipe T into the sterilized fermenting-vat L, whereinit isshowered with its must in the form of rain. The liquor 'to be fermentedis' then introduced through little by little and also in the form thepipe S of rain:

I Second Filtratimt- -When the vat. is full, fermentation is allowed totake place, and then when this is finished the vinous liquid and thevinous liquors are .conducted into a special filterV, which permits the'yeast to be collectedout of contact with theair. This cal bottom havingits top provided, first, with an inlet X for the vinous or fermentedliquors; second, at the center with a stufling-' ,box V, through whichpasses a hollowshaft Y, carrying stirring-arms; third, with an air- Qvalve Z, and,-fourth, with a valved pipe Z communicatingwi th the duct Pfor sterilized air. .In the cylinder is the filter cloth or diaphragm W,which has at center a metallic piece 1, forming a'support to the shaftY.

This piece is hollow and forms a passage for draining 0d the contents ofthe upper compartment, which passage is closed by means of a disk'8 atthe lower end of a rod 2, that extends through the shaft Y to the.ontside, so as to enable the valve-disk 8 to be manipulated. The liquidescapes from the hollow' piece 1 through the orifice 5 in its lower partThe conical part of the filter is also provided with an agitatorcomposed of the hollow shaft 3, having stirring-arms attached andturning about the stationary rod 4, whose upper end is fixed in thepiece 1. The shaft 3 passes through a stufling-bo'x and is providedoutside with a pulley for-rotating the same.

Centralization.flhe liquors which escape from the filter just describedpass into a collecting-vessel W and thence to the dis- The-alcoholproduced by this first distillation is there distilled a second time, ifnecessary, over an acid-salt. f

It only remains to indicate the means for effecting the sterilization ofthe air, the sterilization of the aerator, and the sterilization of thevats.

Sterilization of the air. 'lhe air employed in the whole course ofmanufacture ought, as has been said, to be sterilized. It is sterilizedby passage through an iron coil a, heated in an outside furnace. Thehot. air then passes into and through a vessel 12, provided withdeflecting-partitions and containing sulphuric acid, (H the passagethrough or in filling-column, where they are rendered neu- 'tral orslightly alkaline.

contact with which acidw deprives the air of 1 I the last organizedvgerms which it may still contain. From the vessel 1) the air; passesthrough a cotton filter c, and therein is delivered by appropriate pipesor rluctsto the various apparatus to be supplied therewith.

Sterilization of the aerator.-The inlet-pipe R and the outletS of theliquors being closed, (as also the inlet-pipe K for the sterilized air,)and the communication of the spiralpipes d with the interior of theaerator being established, steam from the'pipe, I-is let into theaerator until all the air is expelled therefrom,

whereupon the stop-cocks in the-pipes dare closed and the steam ismaintained for from ten to fifteen minutes at. a pressure of from two totwo and a'half kilograms. Thus the steam is shit on, the tank cools, andster ilized air ,is' admitted through the after a time fills the tank.

Sterilization of the vats.-The fermentingvat- L is sterilized bybringing waterto a boil therein by means of steam through the pipe 1 Oand perforated pipe N. When the steam IIO pipeK and escapes outside andebullition has been main-- tained forfifteen or twenty minutes, thesupply of steam through pipe 0 is out oif. The

same perforated pipe or distributer N com-.

mlinicates with the pipe P, conveying the sterilized air, and through itthe sterilized air enters. The vat is then ready to receive the must.*

It has been stated that pure yeast is used in the course of the improvedmanufactureand the means for obtaining it have been, de-

scribed. Inasmuch as the wines or vvinous liquids have filtered throughthe filter W and are of a nature to furnish yeast, they leave on-thefilter cloth or diaphragm of the .filter yeast without foreign matter.yThis ,yeast it is intended to put into commerce n. v

the form of pure yeast as a sub-product of the improved manufacture.With this ob ject it is washed two or three times with sterilized must,then with cold sterilized Water, and finally a certain quantity of Verydilute sterilized must is introduced into the filter. The agitator inthe cylinder V is put in motion and the valve-disk 8 is opened, so 'thatthe yeast passes in suspension therein into the conical bottom of saidcylinder. From there it is drawn off by suitable outlets, and with themust introduced into copper bottles of suitable form. J

We claim herein as our invention or discovery- I 1. In the manufactureof alcohol by fermentation and distillation, the improvement consistingin fermenting sterilized mustwith pure yeast out of contact withunsterilized air and subjecting such fermented liquor to distillation,substantially as described.

2. The process of making alcohol, consisting, in sterilizing must,aerating it with sterilized air, fermenting such aerated and sterilizedmust with pure yeast out of contact with unsterilized air, anddistilling such fermented liquor, substantially as described.

3. The process of making alcohol by subjecting must successively tosuperheating, cooling, filtering, aerating, fermenting with "pure yeast,filtering again, and distilling, the operations from the superheating tothe second filtering being carried on out of contact with unsterilizedair, substantially as described.

4. The process of making alcohol by fer menting sterilized must withpure yeast out of contact with unsterili'zed air, separating the yeastout ofcontact with unsterilized air alcohol by fermenting sterilizedmust out of contact with air not sterilized, rendering the anddistilling from such fermented liquor, and distilling,

fermented liquid neutral or slightly alkaline,

the same, substantially as described. 1 j

7; The process of making alcohol by fermenting sterilized must out. ofcontact with air not sterilized, rendering the fermented liquor neutralor. slightly alkaline, distilling off the alcohol from such neutral oralkaline liquor, and redistilling the alcohol over an acid-salt or saltadapted to combine with the ammoniacal bodiesthereof, substantially asdescribed.

8. In apparatus for fermentation and dis tillation, the combination ofthe closed fermenting-vat, the sterilizer for 31138, conduit leadingfrom the latter to the former, a sterile izer for must communicating bya pipe Witli said fermenting-vat, a yeast-vat between the latter and theair-sterilizer and connected with both by pipes or conduits; and anotherpipe for conveyingliquor from the must-steril- 'izer to the yeastat,substantially as described.

9. The combination of the sterilizer for must, the aerator connectedtherewith by a pipe, the air-sterilizer also communicating with saidaerator, the closed fermenting-vat, the pipe connecting the latter withthe aerator and terminating in a sprinkler, the yeast-wit connected by.pipes with the air-sterilizer and aerator, respectively, and connectedwith the fermenting-vat by another pipe, also terminating in asprinkler, substantially as described.

10. The combination of the sterilizer for must, the sterilizer for air,the aerator connected with both by separate pipes, the yeastvatconnected by separate pipes with the aerator and air-sterilizer,respectively, the fermenting-vat connected by pipes with the aerator andyeast-vat, respectively, and the "filter connected with thefermenting-vat, substantially as' described.

. In testimony whereof we have signed this specification in the ingwitnesses.

GASTON GUIGNARD. ANDRE HED UIN. Witnesses:

JOSEPH COURN IER, H R. J. PRESTON.

presence of two subscrib- I

